Process of extracting pine oil, turpentine, and resinous products from wood



ct. 30,1923. f agma T. J. FAIRLEY ET AL PROCESS OF EXTRACTING PINE OIL, TURPENTINE, AND RESINOUS? PRODUCTS FROM WOOD Filed Sept. 2'7 1921 f if;44 /M AW/ Patented Get. 3%, i923.

TALIAFERRO J. FAERLEY AND THOMAS Ill. DU BGSE, GEE HA'E'KIESEUEG, mrssrssrrrr;

SAID DU BOSE ASSIGNOR T0 SAID EAIRLEY.

YROGESS 01E EXTBACTING PINE OIL, TURIEENTINE, AND nnsrn'ous IERQJDUEETQ Fldtllil' WQGD.

' Application filed September 27, E921. denial l lo. fill'ilfifil.

T 0 all whom it may concern Be it known that we, 'lanmrnnao J. Fam- LEY and THOMAS M. DU Boss, citizens of the United states residing at Hattiesburg,

a Forrest County, in the State of Mississippi,

have invented certain new and useful improvements in Processes of Extracting Pine Oil, Turpentine, and Resinous Products from Wood, of which the following is a full,

in clear, and exact specification.

Our invention relates to improvemcntsin the process of extracting certain of the constituent elements of wood by the destructive distillation thereof and the same has for it; its object to provide a simple, convenient and eiiicient process for extracting pine oil, turpentine and other resinous products from wood in greater quantities than has heretofore been possible.

Further, said invention has for its object to provide a process by means of which the production or formation of the noun condensable gases occuring in the processes heretofore known will be wholly prevented, or so reduced in volume as to be negligible.

Further, said invention has for its object to provide a process which is simple to carry out, and by means of which the time necessary for the extraction of the pine oil, turpentine and other resinous products will be greatly shortened, and the cost correspondingly decreased.

Further, said invention has for its object to provide a process whereby a larger yield of pine oil. destructive turpentine and resinous products may be obtained.

Further, said invention has for its object to provide a process which may be carried out at such temperature as to carbonize the wood. and, after removing the excess pine tar oil, leave the carbonized wood soiliciently impregnated or saturated with pine tar oil to permit of the mixture being readily converted into briquettes so as to be as available for fuel purposes.

Other objects will in part be obvious, and in part be pointed out hereinafter.

To the attainment of the aforesaid objects and ends, our invention consists in the process comprising the successive steps hereinafter more fully described and then pointed out in the claims.

The extraction of pine oil, turpentine and other resinous products from. wood has heretofore been accomplished by placing the wood into a closed receptacle having a suitable vapor outlet, and by the application of heat, eithervvithin or without the receptacle, cause the volatile fluids to be vaporized, and then separating the desired W condensate from the remainder thereof; or by placing the wood in a receptacle and subjecting the same to a circulating bath of suitable temperature to extract the desired product, and then separating the some out oi the bath, or by placing the wood in a receptacle and then extracting "the desired products by the use of suitable solvents.

The said processes, however, all require long periods of time to carry out, ranging from thirty to forty-eight hours; yield but a comparatively small volume of the product desired; are all carried out at comparatively low temperatures, and in the case of the first and second named processes result in the production of gases which pass through all forms of condensers without being con densed.

@ur process is principally distinguishable from the processes above specified in that the wood is disposed in a closed container and immersed in a liquid of high boiling point and then subjected to a high temperature which results in the destructive distillation of the wood; prevents the pro duction of vapors which are not condensable; materially reduces the time required for the extraction of the pine oil, turpentine and other resinous products, and finally greatly increases the yield of said products n over that obtained by other recesses.

en destructive distillation of pine wood or the wood of any other tree occurs by the methods at present in use (without the presence of a body of oil surrounding and submerging the wood), it is accompanied by the formation of certain non-condensable gases, which pass through any or all "forms of condensers as a gas or vapor lit) without being condensed into a liquid. The

percentage oi these non-condensable may run as high as twenty per cent tilll itl of the weight of the wood being New, according to our process with all body surrounding the wood in it;

(or such a small amount as till lit

invents negligible) are termed, that are not readily condensed into a liquid by any efficient type of condenser. This may be due to the catalytic action of the oils present by combining certain hydrocarbon groups with the so-called non-condensable gases, after they are formed, into carbon monoxide (CG), carbon dioxide (CO methane (CH,,), and other complex mixtures of the so-called illuminants, having various groupings of carbon (0), oxygen (0) and hydrogen (H), or it may be due to the influence of the oils surrounding the wood chips in preventing the gases formed by the destructive distillation of the wood, from breaking up into non-condensable gases. Whatever the cause may be, however, the presence of the oils in contact with the wood, results in a decided increase in theamount of distillate formed in comparison with any other known process.

The accompanying drawing shows diagrammatically one t'orm of apparatus "for carrying out our process.

In carrying out our process of extract ing pine oil, turpentine and resinous products from long leaf yellow pine and other resinous woods we proceed as follows:

The stumps and down wood are first subjected to the action of a hog, or other suitable apparatus and reduced to chips or particles of the desired degree of fineness.

The chips are then placed in all metal cars or baskets 10, mounted-upon wheels or rollers and introduced into a metal retort 11 which is so mounted in brick work that the same may be heated directly by fire disposed below the same, or preferably, as shown, by a closed steam coil 12 arranged upon or adjacent to the base of the retort 11. The retort is provided at both ends with hinged or removable doors or covers 13, which-may b'e bolted to the ends of the retort so as to form fiuid tight closures.

Pine tar oil, or a suitable mixture of pine tar oil, pine tar, pine oil and turpentine is then introduced from a source of supply it into the retort 11 by a pipe 15 connected to the top of the retort, in sufiicient quantity completely to cover, when heated to a temperature of 600 F. or above, the charge of pine or other resinous wood chips in the retort. The pine tar oil or any mixture thereof, as hereinabove specified, may be in troduced into the retort at atmospheric temperature, or it may be previously heated to any desired temperature. By using pre heated oil the time for distilling the pine wood chips will be materially reduced. Where a plurality of retorts are provided the heated oil maybe withdrawn by a pipe 20 from a retort in which the treatment of a charge of chips has been completed, and conducted to another retort containing a fresh charge of chips to be treate or be pumped directly Saturated or superheated steam, as desired, is then admitted to the steam coils 12, which may be either closed or erforated, to heat the liquid in the retort, 1n order to vaporize the water, and volatile or volatilizable hydrocarbons present in the wood. The produced vapors are conducted by a collector 16 and pipe 17, extending from the top of the retort, to a condenser 18 at any suitable type and size whereby said vapors are efficiently condensed, and the 0ondensate then conducted by a pipe 18 to a suitable gravity separator 19 wherein the oils and lighter liquids will be separated from and floated upon the surface of the water.

When the retort attains a temperature of approximately 200 degrees Fahr. (which is the approximate boiling point of a mixture of water and turpentine), the first vapors are formed and condensed in their passage through the condenser, whence the same pass into and collect in the separator where the oily layer, which is lighter than the water, forms and floats on the surface of the water. 'At first the percentage of oil to water is small, and probably does not exceed five per cent of the water content by volume, but as the distillation proceeds the percentage of oilsincreases until only a trace of water is present in the condensate,

During the first part of the distillation the quantity of low. specific gravity oils is much greater than that of the oils of high s ecific gravity, but towards the end of the distillation the reverse occurs, i. e. the higher specific gravity oils will predominate and only a trace o1 t e low specific gravity oils will he present in the vapors coming over the retort.

While the distillation carried out within a period ranging from six to fourteen hours, and at temperatures ranging from 600 to 1200 degrees Fahrenheit, we find that the results may be best and most economically attained at a term perature of approximately 650 degrees Fahn, or such temperature as ma be necessary not end} completely to V0 atilize all the turpentine and pine oil resent in the wood, but also efficiently to car onize the wood.

When the specific gravity of the combined oils passing from the condenser shows that all pine oil and turpentine have been driven over, and other heavier products are being condensed, the steam supply is shut ofi from the coils, (or the fires drawn if the retort is being heated from without by fire). A valve 21 is then opened so that the original charge of pine tar oil, or any mixture thereof, pumped into the retort, plus a considerable volume of tar, given up by the destructive distillation of the wood may be drawn or by gravity into an auxiliary tank, to the next retort operation may be containing a ilresh charge or chips ready for treatment.

At this stage of the operation there will remain in the retort in the original fireprooi cars or baskets the charcoal thoroughly saturated with the original pine tar oil, plus some tar (formed by the destructive distillation of the wood) which remains behind in the oil, because the temperature within the retort was kept lower than that required to break the tar into tar oil. The end door .or doors 13 of the retort 11 are now opened and the cars containing the oil soaked charcoal are rolled out, leaving the retort empty and ready to receive a fresh charge of chips.

The cars or baskets of oil soaked charcoal are then discharged into a storage hopper for delivery to a briquetting press of proper size to handle the charcoal, which, when freed from oil, amounts to approximately Q00 lbs. per ton (2000 lbs.) of wood treated. During this operation ninety per cent (90%) of the oils present in the charcoal will be extracted, leaving the balance as a hinder to cement the crushed charcoal particles together. The hriquettesthus formed may he used for fuel, either in the plant holler house or sold as fuel to the pulolic.

The distillate from the condenser flows into a gravity separator 19, and inasmuch as water has a specific gravity of 1.000 at 60 F. in comparison with the heaviest weight oils formed during the immersion of the wood chips, with a specific gravity or. under 1.000 at 60 F, the oilwill float on top of the water layer, which latter is drawn oil loy a bottom connection. This water layer which, is sometimes called acid water or pyroligneous acid, actually contains a small amount of wood alcohol, and an average of approximately l.0% acetic acid, both of which may he recovered it desired, but the recovery and refinement is not considered profitalole at the present time.

By the destructive distillation proces es heretolore known or used only an average of less than sixty (60} gallons of crude distillate per ton of wood treated could he produced of which less than eight {8'} gal lens is, turpentine and less than live fttil gallons is pine oil, while hy our process hereinabove described the oils, known as crude oils, are produced in an amount equal to eighty gallons per ton of wood treated, which, when refined will yield about eleven (ll) gallons of wood turpentine, or oils having a specific gravity under .875, twenty-six (26) gallons of pine oil, or oils having a specific gravity under .940 and forty-three (43) gallons of tar, which last named, may he broken down into pine tar oil, if desired.

Having thus described our invention what we claim and desire to secure by Letters Patent is:

1. The process of extracting pine oil, turpentine and resinous products from wood which consists in reducing the wood to chips, immersing said chips in a closed container in a liquid consisting essentially of oils of: the terpene series, subjecting the mass to a temperature of about six hundred degrees Fahrenheit, to effect the destructive distillation of the wood and to convert the volatilizable consitutents of the wood into condensable fluids, condensing; said fluids, and finally separating the aqueous layer from the oleaginous constitutents of the condensate, substantially as specified.

2. The process of extracting pine oil and turpentine from wood which consists in re; ducing the wood to chips, immersing said chips in a closed container in a liquid con sisting essentially of pine tar oil, subjecting the mass to a temperature of six hundred degrees Fahrenheit, to effect the destructive distillation of the wood and to convert the volatilizable constituents of the wood into condensable fluids, condensing said fluids, and finally separating the pine oil, turpentine and resinous matter trom the aqueous layer of the condensate, substantially specified.

3. The process of extracting pine oil, turpentine and resinous products from wood which consists in reducing the wood to chips, immersing said chips in a closed container in a liquid consisting essentially of pine tar oil, subjecting the mass to a temperature or" six hundred degrees Fahrenheit "for a period of approximately six to fourteen hours to ettlect the destructive distillation of the wood and to convert the volatilizahle constitul ents of the wood and said liquid into condensahle fluids, condensing said fluids, and finally separating the pine oil, turpentine and resinous matter from the aqueous-layer of the condensate, suhstantially as specified.

The process of extracting pine oil, pentine and resinous products from wood which consists in reducing; the wood chips, immersing said chips in a closed container in a liquid consisting essentially of pine tax: oil, subjecting the mass to a temperature of sir: hundred degrees Fahrenheit for a period of approximately sir: to fourteen hours to etlect the destructive distillation oi the wood and to convert the volatilisahle constituents oil the wood into condensahie fluids, condensing said fluids, and finally separating the pine oil, turpentine and resinous matter from the aqueous layer of the condensate, substantially as specified.

5. The process of extracting oils of terpene series from wood which consists in reducing the wood to chips, iimnersins; in and subjecting said chips in. a closed con tainer to the action of a catalytic taining an element of a carbonaceous character subjecting the mass to heat to efl'ect the destructive distillation of the Wood and to convert the volatilizable constituents of the wood into condensable fluids, condensing said fluids, and finally separating said oils from the aqueous layer of the condensate, substantially as specified.

6. The process of extracting pine oil, turpentine and resinous products from wood which consists in reducing the wood to chips, immersing and subjecting said chips in a closed container to the action of a liquid containing an element of a carbonaceous character and serving as a catalytic agent, subjecting the mass to heat to effect the destructive distillation of the Wood and to convert the volatilizable constituents of the Wood into condensable fluids, condensing said fluids, and finally separating the pine oil, turpentine and resinous matter from the aqueous layer of the condensate, substantially as specified.

he process of extracting pine oil, turpentine and resinous products from Wood which consists in reducing the Wood to chips, immersing and subjecting said chips in a closed container to the action of a liquid containing an element of a carbonaceous character and serving as a catalytic agent, subjecting the mass to a temperature of ap' proximately six hundred degrees Fahrenheit to effect the destructive distillation of the Wood and-to convert the stituents of the Wood into condensable fluids, condensing said fluids, and finally separating the pine oil, turpentine and resinous matter from the aqueous layer of the condensate, substantially as speci ed.

Signed at Hattiesburg, Forrest County, in the State of Mississippi, this 9th day of September, one thousand nine hundred and twenty-one.

TALIAFERRU J. FAIRLEY. THOMAS M. DU BOSE. Witnesses:

W. Conn COLLINS, Gnssm Roars.

volatilizable con- 

